HRID2198859

反应详情

EQUATION

反应方程式

HRID 2198859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 9.1 parts of 2,3-dimethyl-4-methoxyphenol, 6.5 parts of 1-(tert.-butyl)-3-azetidinol and 0.3 part of potassium hydroxide was heated under nitrogen gas at 140° C. for 8 hours with agitation. The reaction product was dissolved in 100 parts of 2 N-hydrochloric acid aqueous solution and washed twice with 100 parts of ether. The water layer was made alkaline with 4 N-sodium hydroxide aqueous solution, and the resulting crystals were recovered by filtration and dried. Then the crystals were dissolved in 100 parts of ether and decolored. The decolored liquid was concentrated and allowed to cool. As a result, 10.2 parts of 1-(2',3'-dimethyl-4'-methoxyphenoxy)-3-(tert.-butylamino)-2-propanol melting at 73°-75° C. were obtained. The yield was 72.5%. The results of infra-red spectrum analysis and nuclear magnetic resonance analysis of the product are as follows:

WORKUP

后处理

  1. washwashed twice with 100 parts of ether
  2. filtrationthe resulting crystals were recovered by filtration
  3. customdried
  4. dissolutionThen the crystals were dissolved in 100 parts of ether
  5. concentrationThe decolored liquid was concentrated
  6. temperatureto cool